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EC number: 284-366-9
CAS number: 84852-53-9
The combustion samples were analyzed using a VG
Trio-1 GC/MS/DS. Combustion samples were spiked with labeled internal standards
at or below the LOQ for each. Data collected for the labeled PBDD/PBDF
internal standards, which were spiked below target LOQ levels,
demonstrated greater than 10:1 S/N ratios and thus met the Guidelines
sensitivity objective. The Guidelines target that the labeled internal
standards be recovered at 100 +/- 50% was met for 29 of the 32 standards
in the test and quality control samples. Recovery of 13C-2,3,7,8 -TBDF
and 13C-2,3,7,8 -TBDD from Laboratory Method Blank 1 was 44 and 47%,
respectively. Recovery of 13C-2,3,7,8 -PeBDF from test burn PMN-2 was
The reproducibility of the recoveries of the
labeled internal standards from the three incineration experiments
showed a percent relative standard deviation of less than 20%, thus
meeting data quality objectives. Method accuracy was demonstrated by
analyzing two laboratory method blanks that had been fortified with
unlabeled analytes at concentrations at or below the target LOQ.
Recoveries of the spiked analytes from Fortified Laboratory Method Blank
2 ranged from 99 to 140%, which was within the Guidelines targets.
Recoveries of the spiked analytes from fortified Laboratory Method Blank
1 ranged from 100 to 176%. The 176% recovery of 1,2,3,4,7,8 -HxBDF was
the only value outside the Guidelines targest. The recovery of
octabromodibenzodioxin spiked into the Fortified Laboratory Method
Blanks could not be measured.
Analysis of two laboratory method blanks
showed that the equipment and procedures did not contribute
interferences or analytes. Analysis of the background sample showed that
some PBDD/PBDFs were produced by the incinerator itself or were
introduced as contaminants during the analysis. In particular, HpBDF and
HxBDF could be detected, although their concentration appeared to be
considerably below the target LOQ. The quantity of HpBDF and HxBDF did
not affect the test burn results.
The results indicated the combustion
products of DBDPEthane/HIPS/Sb2O3 samples contained no 2,3,7,8
-substituted PBDD/PBDFs at or above the limits of quantitation. One
exception is noted. An adequate detector response could not be
established for octabromodibenzo-p-dioxin at the limit of quantitation
(S/N 10:1). But in all cases the octabromodibenzo-p-dioxin concentration
was below the limit of detection (S/N 3:1).
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